反应详情

温度

0 °C

The material from above 1-(N-benzyloxycarbonyl)-cis-cyclohexane-1,2-diamine (5 g) was dissolved in DMF (100 mL). After cooling to 0° C., 4-methylmorpholine (11 mL) and N-Boc-Gly-OH (4.2 g) were added. BOP Reagent (11.6 g) was added, and the mixture was stirred at rt for 18 h. The DMF was removed. EtOAc was added along with 1 N HCl solution. The EtOAc layer was washed with 1 N HCl, NaHCO3 solution, and brine. The EtOAc was dried (MgSO4), filtered, and concentrated to give cis-[2[[[[(1,1-dimethylethoxy)carbonyl]amino]acetyl]amino]cyclohexyl]-carbamic acid benzyl ester (9.6 g). MS found: (M+H)+=406.3.

1. customThe DMF was removed
2. additionEtOAc was added along with 1 N HCl solution
3. washThe EtOAc layer was washed with 1 N HCl, NaHCO3 solution, and brine
4. dry with materialThe EtOAc was dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated